CN113939736A - Liquefied carbon dioxide supply device and supercritical fluid device - Google Patents
Liquefied carbon dioxide supply device and supercritical fluid device Download PDFInfo
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- CN113939736A CN113939736A CN201980097252.1A CN201980097252A CN113939736A CN 113939736 A CN113939736 A CN 113939736A CN 201980097252 A CN201980097252 A CN 201980097252A CN 113939736 A CN113939736 A CN 113939736A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 206
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 103
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 103
- 239000012530 fluid Substances 0.000 title claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 239000003507 refrigerant Substances 0.000 claims abstract description 20
- 238000005057 refrigeration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000007769 metal material Substances 0.000 claims description 8
- 239000012071 phase Substances 0.000 description 15
- 238000001816 cooling Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 8
- 239000003607 modifier Substances 0.000 description 7
- 238000000194 supercritical-fluid extraction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000011144 upstream manufacturing Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/40—Selective adsorption, e.g. chromatography characterised by the separation mechanism using supercritical fluid as mobile phase or eluent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/16—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
- B01D15/161—Temperature conditioning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3092—Heat exchange between incoming and outgoing mobile phase
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)
Abstract
The liquefied carbon dioxide supply device is configured to supply liquefied carbon dioxide to a supercritical fluid device including a separation column, and includes a first channel section, a second channel section, a compressor, a heat exchanger, and a pump section. The compressor circulates a first refrigerant through the first flow path portion to repeat a refrigeration cycle. The heat exchanger exchanges heat between the first channel portion and the second channel portion. The pump section supplies the liquefied carbon dioxide flowing through the second flow path section to the separation column of the supercritical fluid device.
Description
Technical Field
The present invention relates to a liquid feeding and supplying apparatus for liquefied carbon dioxide and a supercritical fluid apparatus.
Background
In a Supercritical Fluid apparatus such as a Supercritical Fluid Chromatograph (SFC) or a Supercritical Fluid extraction apparatus (Supercritical Fluid Extractor (SFE)), a sample is analyzed or collected using a Supercritical Fluid as a mobile phase. For example, in the SFC described in patent document 1, liquefied carbon dioxide is supplied as a mobile phase to a mobile phase flow path by a liquid-feeding pump. Further, the sample is injected into the mobile phase channel by the sample injection section.
The mobile phase and the sample pass through a separation column disposed in the mobile phase flow path. Here, the pressure in the mobile phase flow path is maintained by a back pressure valve and the temperature of the separation column is maintained by a column oven so that the mobile phase becomes at least in a supercritical state in the separation column. The sample is separated for each sample component by passing through the separation column, and is detected by a detector.
Patent document 1: japanese patent laid-open publication No. 2016-173343
Disclosure of Invention
[ problems to be solved by the invention ]
In a supercritical fluid extraction apparatus, a flow path of carbon dioxide is cooled in order to maintain carbon dioxide in a liquid phase. When the capacity of liquefied carbon dioxide is large, a cooler (chiller) is generally used for cooling the flow path. However, the cooler is relatively large and is mostly installed on the floor. Therefore, the installation space for the cooler becomes large, and the supercritical fluid apparatus becomes large. Further, since the piping is indirectly cooled using a refrigerant such as water, the temperature of the liquefied carbon dioxide cannot be stably controlled. In this case, as the density of the liquefied carbon dioxide becomes unstable, the flow rate of the liquefied carbon dioxide becomes unstable.
The purpose of the present invention is to provide a liquefied carbon dioxide liquid-feeding supply device and a supercritical fluid device capable of supplying liquefied carbon dioxide at a stable flow rate while suppressing an increase in size.
[ means for solving problems ]
An aspect according to an aspect of the present invention relates to a liquefied carbon dioxide supply apparatus that supplies liquefied carbon dioxide to a supercritical fluid apparatus including a separation column, the liquefied carbon dioxide supply apparatus including: a first channel section and a second channel section; a compressor that circulates a first refrigerant through the first channel portion to repeat a refrigeration cycle; a heat exchanger that exchanges heat between the first channel portion and the second channel portion; and a pump section for supplying the liquefied carbon dioxide flowing through the second channel section to the separation column.
[ Effect of the invention ]
According to the present invention, liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in size of the liquefied carbon dioxide liquid supply and supply device and the supercritical fluid device.
Drawings
Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention.
Fig. 2 is a diagram showing a configuration of the liquefied carbon dioxide supply device of fig. 1.
Detailed Description
(1) Structure of supercritical fluid device
Hereinafter, a liquefied carbon dioxide liquid feeding and supplying apparatus and a supercritical fluid apparatus according to an embodiment of the present invention will be described in detail with reference to the drawings. Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention. As shown in fig. 1, the supercritical fluid apparatus 200 is a Supercritical Fluid Chromatograph (SFC) including: a liquefied carbon dioxide supply device 100, a modifier (modifier) supply device 110, a mixing unit 120, a sample supply unit 130, a separation column 140, a detector 150, a back pressure valve 160, and a control unit 170.
In the bottle 202, a modifier such as an organic solvent is stored as a mobile phase. Modifier supply device 110 is, for example, a liquid feeding pump, and pumps modifier stored in bottle 202 under pressure. The mixing section 120 is, for example, a gradient mixer (gradient mixer) and supplies the mobile phases pumped and supplied from the liquefied carbon dioxide supply apparatus 100 and the modifier supply apparatus 110 at a predetermined ratio while mixing them.
The sample supply unit 130 is, for example, an ejector (injector), and introduces a sample to be analyzed and the mobile phase supplied from the mixing unit 120 into the separation column 140. The separation column 140 is housed in a column thermostat, not shown, and is heated to a predetermined temperature (about 40 ℃ in the present example) so that the liquefied carbon dioxide in the introduced mobile phase is in a supercritical state. The separation column 140 separates the introduced sample into components according to the difference in chemical properties or composition.
The detector 150 is, for example, an absorbance detector, and detects components of the sample separated by the separation column 140. The detection result obtained by the detector 150 is used to generate, for example, a supercritical fluid chromatogram showing the relationship between the retention time and the detection intensity of each component. The back pressure valve 160 maintains the pressure in the flow path of the mobile phase at a pressure equal to or higher than the critical pressure of carbon dioxide (for example, 8MPa) so that the liquefied carbon dioxide in the mobile phase is in a supercritical state at least in the separation column 140.
The control Unit 170 includes a Central Processing Unit (CPU), a memory, a microcomputer, or the like, and controls the operations of the liquefied carbon dioxide supply device 100, the modifier supply device 110, the mixing Unit 120, the sample supply Unit 130, the separation column 140 (column thermostat), the detector 150, and the back pressure valve 160. In the case where a separator such as a fraction collector (fraction collector) is provided downstream of the back pressure valve 160, the control unit 170 further controls the operation of the separator based on the detection result obtained by the detector 150. The control unit 170 may be provided in the back pressure valve 160.
(2) Structure of liquefied carbon dioxide supply device
Fig. 2 is a diagram showing a configuration of the liquefied carbon dioxide supply apparatus 100 shown in fig. 1. As shown in fig. 2, the liquefied carbon dioxide supply device 100 includes a cooling unit 10 and a pump unit 20. The liquefied carbon dioxide supply device 100 is provided with a flow path unit 1, a flow path unit 2, and a flow path unit 3. The flow path portions 1 to 3 are, for example, pipes. The flow path portions 1 to 3 are examples of first to third flow path portions, respectively. In the following description, the flow path section 2 and the flow path section 3 define the direction in which the liquefied carbon dioxide or the refrigerant flows as the downstream direction, and the opposite direction as the upstream direction.
The cooling portion 10 includes: heat exchanger 11, compressor 12, reservoir 13, and liquid feed 14. The heat exchanger 11 includes a block portion 11a and a metal material 11 b. The block 11a includes four side surfaces, an upper surface, and a bottom surface formed of a metal plate, and has a rectangular parallelepiped shape. The block 11a accommodates a part of each of the flow path section 1, the flow path section 2, and the flow path section 3. The metal material 11b contains, for example, tin, and is filled into the block portion 11a in a molten state. Thus, in the block 11a, gaps among the flow path section 1, the flow path section 2, and the flow path section 3 are filled with the metal material 11 b.
Both ends of the flow path portion 1 are drawn out from the block portion 11a and connected to the compressor 12. The compressor 12 circulates a refrigerant such as fluorocarbon 407C (R-407C) through the flow path portion 1 to repeat the refrigeration cycle. Thereby, the inside of the block portion 11a is cooled. In this example, the flow path section 1 is provided in the block section 11a in a state of being wound in a coil shape. Therefore, even when the sufficiently long flow path section 1 is used, the block section 11a is maintained compact. Therefore, by using the sufficiently long flow path section 1, the inside of the block section 11a can be sufficiently cooled.
The flow path section 2 connects the bottle 201 and the mixing section 120. The heat exchanger 11 and the pump unit 20 are inserted into the flow path portion 2 from upstream to downstream. In the block portion 11a, heat is exchanged between the flow path portion 1 and the flow path portion 2 via the metal material 11 b. Thereby, the liquefied carbon dioxide supplied from bottle 201 to mixing unit 120 is cooled. In this example, the flow path section 2 is provided so as to meander within the block section 11 a. Therefore, the portion of the flow path section 2 provided in the block section 11a can be made long. Therefore, the liquefied carbon dioxide can be sufficiently cooled.
The storage unit 13 is, for example, a bottle, and stores a refrigerant such as ethylene glycol having a concentration of 60%. The liquid feeding unit 14 is, for example, a diaphragm pump (diaphragm pump), and pumps the refrigerant stored in the storage unit 13 to the pump unit 20 through the channel unit 3. The heat exchanger 11 is inserted into a portion of the channel section 3 between the liquid feeding section 14 and the pump section 20. In the block portion 11a, heat is exchanged between the flow path portion 1 and the flow path portion 3 via the metal material 11 b. Thereby, the refrigerant supplied from the liquid feeding portion 14 to the pump portion 20 is cooled. The refrigerant supplied to the pump unit 20 passes through the channel unit 3 and returns to the reservoir unit 13.
In this example, the pump section 20 is a parallel plunger pump, and includes two pump heads 21 and 22. In the pump section 20, the channel section 2 includes a main channel section 2a, a main channel section 2b, a branch channel section 2c, and a branch channel section 2 d. The main channel portion 2a and the main channel portion 2b are connected to the cooling portion 10 and the mixing portion 120, respectively. The branch channel part 2c and the branch channel part 2d are disposed in parallel so as to branch into two channels between the main channel part 2a and the main channel part 2 b. The pump head 21 and the pump head 22 are inserted into the branch flow path part 2c and the branch flow path part 2d, respectively, and the liquefied carbon dioxide stored in the bottle 201 is alternately pressure-fed to the mixing part 120 through the cooling part 10.
In the pump section 20, the channel section 3 includes a main channel section 3a, a main channel section 3b, a branch channel section 3c, and a branch channel section 3 d. The main flow path portion 3a and the main flow path portion 3b are connected to the heat exchanger 11 and the reservoir portion 13 of the cooling unit 10, respectively. The branch flow path section 3c and the branch flow path section 3d are disposed in parallel so as to branch into two flow paths between the main flow path section 3a and the main flow path section 3b, and are attached to the surfaces of the pump heads 21 and 22, respectively. The refrigerant supplied from the heat exchanger 11 through the main channel portion 3a flows through the branch channel portion 3c and the branch channel portion 3 d. Thereby, the pump heads 21 and 22 are cooled. The refrigerant flowing through the branch flow path portion 3c and the branch flow path portion 3d passes through the main flow path portion 3b and returns to the reservoir portion 13.
(3) Operation of the control section
According to the cooling mechanism, in the heat exchanger 11, the flow path section 1 is cooled to, for example, about-30 ℃, and the flow path sections 2 and 3 are cooled to, for example, about-10 ℃. On the other hand, the temperature of the liquefied carbon dioxide flowing through the passage portion 2 is preferably other values (about 5 ℃ in the present example). The temperatures of the pump heads 21 and 22 are preferably other values (about 5 ℃ in this example).
Therefore, the heating unit 15 and the heating unit 16 are attached to the downstream portions of the flow path section 2 and the flow path section 3, respectively, which are drawn out from the block 11 a. The heating unit 15 and the heating unit 16 are examples of a first heating unit and a second heating unit, respectively. Further, a temperature sensor 4 is mounted on the surface of the flow path portion 2 downstream of the heating portion 15. Further, a temperature sensor 5 and a temperature sensor 6 are attached to the surfaces of the pump heads 21 and 22, respectively. The temperature sensors 4 to 6 each include, for example, a thermistor (thermistor). The temperature sensor 4 is an example of a first temperature sensor, and the temperature sensors 5 and 6 are examples of a second temperature sensor. The operations of the heating portions 15 and 16 are independently controlled by the control portion 170 of fig. 1.
Specifically, the operation of the heating portion 15 is controlled so that the temperature detected by the temperature sensor 4 becomes a desired temperature. Here, since the temperature sensor 4 is directly attached to the surface of the flow path unit 2, the temperature of the liquefied carbon dioxide flowing through the flow path unit 2 is accurately detected as the temperature of the flow path unit 2. Therefore, the temperature of the liquefied carbon dioxide flowing through the flow path portion 2 can be maintained at a desired temperature by the control. The temperature sensor 4 can be fixed to the flow path portion 2 by an electrically conductive adhesive tape or an electrically conductive adhesive having high thermal conductivity. In this case, the temperature of the flow path section 2 can be detected with higher accuracy.
Similarly, the operation of the heating unit 16 is controlled so that the temperatures detected by the temperature sensors 5 and 6 become desired temperatures. This can maintain the temperature of the pump heads 21 and 22 at a desired temperature. The temperature sensors 5 and 6 may be directly attached to the surfaces of the branch flow path section 3c and the branch flow path section 3d, and the temperatures of the pump head 21 and the pump head 22 may be detected as the temperatures of the branch flow path section 3c and the branch flow path section 3d, respectively.
(4) Effect
In the supercritical fluid apparatus 200 according to the present embodiment, since it is not necessary to use a cooler for cooling the flow path section 2, the size increase of the liquefied carbon dioxide supply apparatus 100 is suppressed. In this case, the liquefied carbon dioxide supply device 100 may be mounted on a table, rather than on a floor. Therefore, a wide space can be secured in the supercritical fluid apparatus 200, and space can be saved.
Further, the flow path portion 2 can be directly cooled without using a refrigerant such as water. Therefore, the temperature of the liquefied carbon dioxide becomes stable, and thereby the density of the liquefied carbon dioxide becomes stable. As a result, liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in size of the liquefied carbon dioxide supply apparatus 100 and the supercritical fluid apparatus 200.
The flow path section 2 is heated by the heating section 15 based on the temperature detected by the temperature sensor 4. Here, since the temperature sensor 4 is directly attached to the surface of the flow path unit 2, the temperature of the flow path unit 2 can be accurately detected as the temperature of the liquefied carbon dioxide flowing through the flow path unit 2. Therefore, the temperature of the liquefied carbon dioxide can be easily adjusted to a desired temperature. This makes it possible to supply liquefied carbon dioxide at a more stable flow rate.
When the flow rate of the liquefied carbon dioxide is small, the temperature of the liquefied carbon dioxide is likely to fluctuate in the portion of the flow path section 2 from the heat exchanger 11 to the pump section 20 due to the influence of the outside air. In this case, heat is also exchanged between the flow path section 1 and the flow path section 3 by the heat exchanger 11. Further, based on the temperatures of the pump head 21 and the pump head 22 detected by the temperature sensor 5 and the temperature sensor 6, respectively, the temperature of the flow path section 3 is adjusted by the heating section 16 so as to be a desired temperature. Thereby, the pump heads 21 and 22 are cooled to a desired temperature via the refrigerant flowing through the flow path section 3. As a result, the temperature of the liquefied carbon dioxide supplied from the pump section 20 can be further stabilized.
(5) Other embodiments
(a) In the above embodiment, the cooling unit 10 is configured to be able to cool the pump head 21 and the pump head 22 of the pump unit 20, but the embodiment is not limited thereto. The cooling unit 10 may not be configured to be able to cool the pump head 21 and the pump head 22 of the pump unit 20 when the temperatures of the pump head 21 and the pump head 22 are sufficiently stable or when the temperatures of the pump head 21 and the pump head 22 are adjusted by another temperature adjustment device.
(b) In the above embodiment, the heating portion 15 is attached to the downstream portion of the flow path portion 2 drawn out from the block portion 11a, but the embodiment is not limited thereto. The heating section 15 may be installed in an upstream portion of the flow path section 2 drawn from the block section 11 a. In this case, the temperature sensor 4 is also attached to the flow path section 2 further downstream than the heat exchanger 11 and the heating section 15.
Similarly, the heating unit 16 is attached to a downstream portion of the flow path unit 3 drawn out from the block 11a, but the embodiment is not limited thereto. The heating section 16 may be installed in an upstream portion of the flow path section 3 drawn from the block section 11 a.
When the liquefied carbon dioxide flowing through the flow path section 2 is cooled to a desired temperature by the heat exchanger 11, the heating section 15 may not be attached to the flow path section 2. When the pump head 21 and the pump head 22 are cooled to a desired temperature by the heat exchanger 11, the heating unit 16 may not be attached to the flow path section 3.
(c) In the above embodiment, the supercritical fluid apparatus 200 is configured as SFC, but the embodiment is not limited thereto. Supercritical fluid apparatus 200 may also be configured as a supercritical fluid extraction apparatus (SFE). Alternatively, the supercritical fluid apparatus 200 may be configured to include a Mass Spectrometer (MS) instead of the SFC-MS of the detector 150.
(6) Form of the composition
The liquefied carbon dioxide supply device according to the (item 1) above
Supplying liquefied carbon dioxide to a supercritical fluid apparatus including a separation column, the liquefied carbon dioxide supply apparatus including:
a first channel section and a second channel section;
a compressor that circulates a first refrigerant through the first channel portion to repeat a refrigeration cycle;
a heat exchanger that exchanges heat between the first channel portion and the second channel portion; and
and a pump section for supplying the liquefied carbon dioxide flowing through the second channel section to the separation column.
In the liquefied carbon dioxide supply device, the first refrigerant is circulated through the first flow path unit by the compressor so that the refrigeration cycle is repeated. In this case, in the heat exchanger, heat is exchanged between the first channel portion and the second channel portion, and the second channel portion is cooled. Therefore, the liquefied carbon dioxide flowing through the second flow path portion is cooled. The liquefied carbon dioxide cooled in the second channel section is supplied to the separation column of the supercritical fluid device by the pump section.
According to the above configuration, since it is not necessary to use a cooler for cooling the second flow path portion, the size of the liquefied carbon dioxide supply device can be suppressed from increasing. Further, the second channel portion can be directly cooled without using a refrigerant such as water. Therefore, the temperature of the liquefied carbon dioxide becomes stable, and thereby the density of the liquefied carbon dioxide becomes stable. As a result, the liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in the size of the liquefied carbon dioxide supply device.
(item 2) the liquefied carbon dioxide supply apparatus according to item 1, may be
The heat exchanger includes:
a block portion having an internal space for accommodating a part of the first channel portion and a part of the second channel portion; and
and a metal material filled in the internal space of the block portion so as to fill a gap between the first channel portion and the second channel portion.
In this case, heat can be efficiently exchanged between the first channel portion and the second channel portion via the metal material.
(item 3) the liquefied carbon dioxide supply apparatus according to item 1 or 2, wherein
Further, the apparatus includes a first heating unit that heats the second channel unit.
In this case, the temperature of the second channel portion can be easily maintained at a desired temperature by heating the second channel portion. This allows the liquefied carbon dioxide flowing through the second flow path portion to be maintained at a desired temperature.
(item 4) the liquefied carbon dioxide supply apparatus according to item 3, may be
The heat exchanger further includes a first temperature sensor that is attached to the second flow path portion and detects a temperature of the second flow path portion, downstream of the heat exchanger and the first heating unit.
In this case, since the first temperature sensor is attached to the second channel portion, the temperature of the second channel portion can be accurately detected as the temperature of the liquefied carbon dioxide flowing through the second channel portion. Therefore, the temperature of the liquefied carbon dioxide flowing through the second flow path portion can be easily adjusted by the first heating unit based on the detected temperature. This makes it possible to supply liquefied carbon dioxide at a more stable flow rate.
(item 5) the liquefied carbon dioxide supply apparatus according to item 1 or 2, wherein
Further comprises a third flow path part for circulating the second refrigerant,
the heat exchanger further exchanges heat between the first flow path portion and the third flow path portion,
the pump section includes a pump head to which a part of the third channel section is attached.
When the flow rate of the liquefied carbon dioxide is small, the temperature of the liquefied carbon dioxide is likely to vary in the portion from the heat exchanger to the second channel portion of the pump portion due to the influence of the outside air. In this case, according to the above configuration, the pump head is also cooled by the third flow path portion. This makes it possible to further stabilize the temperature of the liquefied carbon dioxide supplied from the pump unit.
(item 6) the liquefied carbon dioxide supply apparatus according to item 5, wherein
Further, the apparatus includes a second heating unit that heats the third channel unit.
In this case, the temperature of the third channel part can be easily maintained at a desired temperature by heating the third channel part. Thus, the temperature of the pump head can be maintained at a desired temperature via the second refrigerant flowing through the third flow path portion. As a result, the temperature of the liquefied carbon dioxide supplied from the pump section can be maintained at a desired temperature.
(item 7) the liquefied carbon dioxide supply apparatus according to item 6, wherein
Further comprising a second temperature sensor for detecting the temperature of the pump head.
In this case, the temperature of the third flow path section can be easily adjusted by the second heating unit based on the temperature detected by the second temperature sensor.
The supercritical fluid apparatus according to another aspect (item 8) may include:
a separation column;
the liquefied carbon dioxide supply device according to claim 4, wherein the separation column is supplied with liquefied carbon dioxide; and
and a control unit that controls an operation of the first heating unit such that a temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature.
In the supercritical fluid apparatus, the operation of the first heating unit is controlled by the control unit so that the temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature. Thereby, the temperature of the liquefied carbon dioxide flowing through the second flow path portion is maintained at a desired temperature. According to this configuration, the liquefied carbon dioxide can be supplied to the separation column at a more stable flow rate while suppressing an increase in size of the liquefied carbon dioxide supply device.
Claims (8)
1. A liquefied carbon dioxide supply device that supplies liquefied carbon dioxide to a supercritical fluid device including a separation column, the liquefied carbon dioxide supply device comprising:
a first channel section and a second channel section;
a compressor that circulates a first refrigerant through the first channel portion to repeat a refrigeration cycle;
a heat exchanger that exchanges heat between the first channel portion and the second channel portion; and
and a pump section for supplying the liquefied carbon dioxide flowing through the second channel section to the separation column.
2. The liquefied carbon dioxide supply apparatus according to claim 1, wherein the heat exchanger includes:
a block portion having an internal space for accommodating a part of the first channel portion and a part of the second channel portion; and
and a metal material filled in the internal space of the block portion so as to fill a gap between the first channel portion and the second channel portion.
3. The liquefied carbon dioxide supply device according to claim 1 or 2, further comprising a first heating unit that heats the second flow path unit.
4. The liquefied carbon dioxide supply device according to claim 3, further comprising a first temperature sensor that is attached to the second flow path section and detects the temperature of the second flow path section, further downstream of the heat exchanger and the first heating section.
5. The liquefied carbon dioxide supply device according to claim 1 or 2, further comprising a third flow path portion through which the second refrigerant circulates,
the heat exchanger further exchanges heat between the first flow path portion and the third flow path portion,
the pump section includes a pump head to which a part of the third channel section is attached.
6. The liquefied carbon dioxide supply device according to claim 5, further comprising a second heating unit that heats the third flow path unit.
7. The liquefied carbon dioxide supply device according to claim 6, further comprising a second temperature sensor that detects a temperature of the pump head.
8. A supercritical fluid apparatus comprising:
a separation column;
the liquefied carbon dioxide supply device according to claim 4, wherein the separation column is supplied with liquefied carbon dioxide; and
and a control unit that controls an operation of the first heating unit such that a temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2019/023156 WO2020250317A1 (en) | 2019-06-11 | 2019-06-11 | Liquefied carbon dioxide feeding device and supercritical fluid apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113939736A true CN113939736A (en) | 2022-01-14 |
| CN113939736B CN113939736B (en) | 2024-06-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201980097252.1A Active CN113939736B (en) | 2019-06-11 | 2019-06-11 | Liquefied carbon dioxide supply device and supercritical fluid device |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US12044662B2 (en) |
| JP (1) | JP7342946B2 (en) |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN113939736B (en) | 2024-06-25 |
| JP7342946B2 (en) | 2023-09-12 |
| US20220229024A1 (en) | 2022-07-21 |
| JPWO2020250317A1 (en) | 2020-12-17 |
| WO2020250317A1 (en) | 2020-12-17 |
| US12044662B2 (en) | 2024-07-23 |
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